CN108653369A - A kind of preparation method of honeysuckle extractive of general flavone and its application in honey refines emblic loquat leaf extract - Google Patents
A kind of preparation method of honeysuckle extractive of general flavone and its application in honey refines emblic loquat leaf extract Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/35—Caprifoliaceae (Honeysuckle family)
- A61K36/355—Lonicera (honeysuckle)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
Application the invention discloses a kind of preparation method of honeysuckle extractive of general flavone and its in honey refines emblic loquat leaf extract.The step of preparation method, is as follows：1）Honeysuckle crushed 30 mesh；2）Petroleum ether degreasing is added；3）It filters, filter residue volatilizes；4）Ethanol solution, assisted microwave synthesis extraction is added；5）Solution filtering is concentrated and dried；6）By the purifying water dissolution of the crude product after drying, D101 macroporous absorbent resins, ethanol solution elution are crossed.7）Eluent concentrates, freeze-drying.The method of the present invention is easy to operate, and solvent dosage is small, and environmental pollution is small；It can be recycled using ethyl alcohol extraction and macroreticular resin, reduce cost, economize on resources.The honeysuckle extractive of general flavone prepared using this method has stronger inhibiting effect in honey refines emblic loquat leaf extract to the proliferation of myocardial fibrosis cell.
Description
Technical field
The invention belongs to traditional Chinese medicine extraction and application field more particularly to a kind of preparation methods of honeysuckle extractive of general flavone
And its application in honey refines emblic loquat leaf extract.
Background technology
Honey refining emblic loquat leaf extract has moistening lung for removing phlegm, relieving cough and asthma, clearing heat and cooling blood, aligning fall fire and other effects, mainly contains
There are loquat, emblic, honeysuckle isoreactivity ingredient.Honeysuckle also known as honeysuckle, it is clearing heat and detoxicating that numerous studies show that honeysuckle has
And other effects, it is famous one of the Chinese herbal medicine in China, has the medication history of more than one thousand years, planted extensively in China.Honeysuckle contains
The multiple compounds such as organic acid, polysaccharide, flavonoids, volatile oil.In recent years, with to honeysuckle in-depth study, Ren Menfa
Flavone compound in cash honeysuckle flower has very high researching value, antibacterial, antiviral, strengthen immunity, anti-cancer and cancer-preventing,
Myocardial preservation etc. has significant curative effect.The active ingredient for having developed and used flavones in honeysuckle has important economic value
And social benefit.The present invention evaluates extracted general flavone and exists by improving the recovery rate with general flavone in improvement honeysuckle
Effect in terms of myocardial fibrosis cell improvement has the function of a variety of heart diseases such as medical treatment myocardial fibrosis positive.
Currently, related gold and silver flower flavone extraction process and its application study are less, present invention combination traditional handicraft and modern crafts, carefully
Change technological parameter, extraction when assisted microwave synthesis extract, technique have high selectivity, the operating time is short, solvent consumption is small, effective
The high feature of ingredient yield.
Invention content
The present invention provides the extraction of general flavone in honeysuckle and applications.The present invention mutually ties traditional handicraft with modern crafts
It closes, process for refining parameter, in extraction, assisted microwave synthesis extracts, and technique has that high selectivity, operating time be short, solvent consumption
The characteristics of small, active ingredient high income.
In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions：
A kind of preparation method of honeysuckle extractive of general flavone, includes the following steps：
（1）Raw material is handled, honeysuckle is crushed using Universalpulverizer, crosses 30 mesh screens；
（2）Petroleum ether is added according to solid-liquid ratio to be uniformly mixed, degreasing 30 minutes；
（3）Feed liquid after degreasing is filtered, filter residue volatilizes；
（4）Ethanol solution, assisted microwave synthesis ultrasonic extraction are added in the filter residue volatilized；
（5）Ethanol extract is merged and is filtered, filtrate concentration is in paste, and chromocor compound crude product is freeze-dried to obtain at -80 DEG C；
（6）Chromocor compound crude product is dissolved in purified water, concentration 40mg/ml crosses the ethyl alcohol that 2~3 times of wet resin volumes are added in column
Solution elutes, 1.2~1.5ml/min of flow velocity, room temperature elution；
（7）By the solution decompression or vacuum concentration after elution, the solution after concentration is freeze-dried 18~24 hours at -80 DEG C and makes
Obtain honeysuckle extractive of general flavone.
Preferably, the step（2）The solid-liquid ratio of middle honeysuckle and petroleum ether is 1：10~1:20（g/ml）.
Preferably, the step（4）Middle filter residue is 1 with ethyl alcohol solid-liquid ratio:10~1:25（g/ml）.
Preferably, the step（4）Middle ethanol solution concentration is 40%~80%.
Preferably, the step（4）Middle to be extracted using Microwave-Assisted Ethanol solution, microwave temperature is 30~60
DEG C, microwave irradiation time 30~75 minutes.
Preferably, the step（4）Middle to be extracted using Microwave-Assisted Ethanol solution, Microwave Extraction number is 2 ~ 3 times.
Preferably, the step（5）Middle filtrate is concentrated using vacuum or condition of negative pressure, and vacuum degree is -0.085~
0.09MPa。
Preferably, the step（5）Middle filtrate is concentrated into the 20%~30% of material liquid.
Preferably, the step（6）Middle chromocor compound crude product is eluted using D101 macroreticular resins.
Preferably, the step（6）Middle chromocor compound crude product is eluted using 75% ~ 85% ethyl alcohol.
The method of the present invention is simple and easy to do, compared with prior art, a kind of honeysuckle extractive of general flavone described in this patent
Preparation method and application have the advantages that.Traditional handicraft is combined by the present invention with modern crafts, molten using ethyl alcohol
Liquid extracts, and in extraction, assisted microwave synthesis extracts, and the operating time is short, and general flavone yield improves；Solvent dosage is reduced, macroreticular resin can
Cycle is used for multiple times, and reduces cost, reduces the pollution to environment.More than honeysuckle extractive of general flavone prepared by the present invention is refined in honey
The stronger inhibited proliferation to myocardial fibrosis cell has been played in sweet sub- loquat leaf extract.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, but embodiment is not to technical solution of the present invention
It limits, it is all based on present invention teach that made variation or equivalent replacement, is within the scope of protection of the invention.
Embodiment one
Raw material is handled, honeysuckle is crushed using Universalpulverizer, crosses 30 mesh screens；According to solid-liquid ratio 1：10（g/ml）
Petroleum ether is added to be uniformly mixed, degreasing 30 minutes；Feed liquid after degreasing is filtered, filter residue volatilizes；In the filter residue volatilized
According to solid-liquid ratio 1：10（g/ml）40% ethanol solution is added to extract, extraction process uses microwave radiation technology, controls microwave temperature
30 DEG C, microwave extraction 30 minutes extracts 2 times；Ethanol extract is merged and is filtered, filtrate is 0.09MPa's in vacuum degree
Under the conditions of be concentrated into the 20% of material liquid, be in paste, chromocor compound crude product is freeze-dried to obtain at -80 DEG C；By chromocor compound
Crude product is dissolved in purified water, and concentration 40mg/ml crosses D101 macroporous absorbent resins.2~3 times of 75% ethanol solutions of wet resin volume are added
Elution, 1.2~1.5ml/min of flow velocity, room temperature elution；Solution decompression after elution or vacuum concentration, the solution after concentration is -80
It is freeze-dried 18 hours at DEG C, obtains honeysuckle extractive of general flavone, extract yield 4.87%, general flavone purity 83.3%.
Embodiment two
Raw material is handled, honeysuckle is crushed using Universalpulverizer, crosses 30 mesh screens；According to solid-liquid ratio 1：15（g/ml）
Petroleum ether is added to be uniformly mixed, degreasing 30 minutes；Feed liquid after degreasing is filtered, filter residue volatilizes；In the filter residue volatilized
According to solid-liquid ratio 1：15（g/ml）60% ethanol solution is added to extract, extraction process uses microwave radiation technology, controls microwave temperature
40 DEG C, microwave extraction 45 minutes extracts 3 times；Ethanol extract is merged and is filtered, negative pressure item of the filtrate in -0.085MPa
It is concentrated into the 30% of material liquid under part, is in paste, chromocor compound crude product is freeze-dried to obtain at -80 DEG C；Chromocor compound is thick
Product are dissolved in purified water, and concentration 40mg/ml crosses D101 macroporous absorbent resins.2~3 times of 85% ethanol solutions of wet resin volume are added to wash
It is de-, 1.2~1.5ml/min of flow velocity, room temperature elution；Solution decompression after elution or vacuum concentration, the solution after concentration is at -80 DEG C
Lower freeze-drying 24 hours, obtains honeysuckle extractive of general flavone, extract yield 5.21%, general flavone purity 85.4%.
Embodiment three
Raw material is handled, honeysuckle is crushed using Universalpulverizer, crosses 30 mesh screens；According to solid-liquid ratio 1：20（g/ml）
Petroleum ether is added to be uniformly mixed, degreasing 30 minutes；Feed liquid after degreasing is filtered, filter residue volatilizes；In the filter residue volatilized
According to solid-liquid ratio 1：25（g/ml）80% ethanol solution is added to extract, extraction process uses microwave radiation technology, controls microwave temperature
60 DEG C, microwave extraction 60 minutes extracts 3 times；Ethanol extract is merged and is filtered, filtrate is 0.09MPa in vacuum degree,
Under the conditions of be concentrated into the 20% of material liquid, be in paste, chromocor compound crude product is freeze-dried to obtain at -80 DEG C；By chromocor compound
Crude product is dissolved in purified water, and concentration 40mg/ml crosses D101 macroporous absorbent resins.2~3 times of 85% ethanol solutions of wet resin volume are added
Elution, 1.2~1.5ml/min of flow velocity, room temperature elution；Solution decompression after elution or vacuum concentration, the solution after concentration is -80
It is freeze-dried 24 hours at DEG C, obtains honeysuckle extractive of general flavone, extract yield 5.14%, general flavone purity 82.6%.
Example IV
Raw material is handled, honeysuckle is crushed using Universalpulverizer, crosses 30 mesh screens；According to solid-liquid ratio 1：20（g/ml）
Petroleum ether is added to be uniformly mixed, degreasing 30 minutes.Feed liquid after degreasing is filtered, and filter residue volatilizes spare.In the filter residue volatilized
According to solid-liquid ratio 1：20（g/ml）The ethanol water of addition 60% extracts, assisted microwave synthesis ultrasound, 40 DEG C of microwave temperature,
Microwave irradiation time 45 minutes extracts 2 times.Ethanol water after extraction, which merges, to be filtered, and filtrate is in -0.085MPa condition of negative pressure
Under be concentrated into the 30% of material liquid, be in paste, chromocor compound crude product is freeze-dried to obtain at -80 DEG C.Chromocor compound crude product is molten
In purified water, D101 macroporous absorbent resins are crossed.2~3 times of 75% ethanol waters of wet resin volume are added to elute, flow velocity 1.2~
1.5ml/min, room temperature elution.Solution decompression after elution is concentrated in vacuo, and it is small that the solution after concentration is freeze-dried 18 at -80 DEG C
When, obtain honeysuckle extractive of general flavone, extract yield 5.37%, general flavone purity 86.6%.
Active testing extract obtained embodiment 1-4
Separation, culture rat myocardial fibroblasts, are divided into myocardial fibrosis group, honeysuckle extractive of general flavone group, take logarithm
The myocardial fibrosis cell in growth period presses cell suspension per hole 1 × 104A cell inoculation is in 96 orifice plates, 37 DEG C, 5%
CO2And cultivated under saturated humidity and change serum free medium afterwards for 24 hours, after continuing culture for 24 hours, cell is made to enter growth resting stage.It inhales
Each hole culture medium is abandoned, blank cultures, honeysuckle extractive of general flavone low, middle and high dose groups difference is added in myocardial fibrosis group
It is added and contains 200 μ g.mL-1、400μg.mL-1、600μg.mL-1Extractive of general flavone, continue to cultivate, 96 holes taken out after 48h
20 μ L of CCK-8 solution are added per hole for plate, continue to be incubated 30min.Microplate reader measures the light absorption value in each hole at 450nm（A）, calculate
Inhibiting rate the results are shown in Table 1.
The influence that 1 honeysuckle extractive of general flavone of table is proliferated rat myocardial fibroblasts（n=6）
As can be seen from Table 1, proliferation of the honeysuckle extractive of general flavone to myocardial fibrosis cell in honey refining emblic loquat leaf extract
It significantly inhibits.
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention,
Obviously the present invention specific implementation is not subject to the restrictions described above, as long as use the inventive concept and technical scheme of the present invention into
The improvement of capable various unsubstantialities, or it is not improved by the present invention design and technical solution directly apply to other occasions
, within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of honeysuckle extractive of general flavone, it is characterised in that include the following steps：
（1）Raw material is handled, honeysuckle is crushed using Universalpulverizer, crosses 30 mesh screens；
（2）Petroleum ether is added into honeysuckle to be uniformly mixed, degreasing 30 minutes；
（3）Feed liquid after degreasing is filtered, filter residue volatilizes；
（4）Ethanol solution, assisted microwave synthesis ultrasonic extraction are added in the filter residue volatilized；
（5）Ethanol extract is merged and is filtered, filtrate concentration is in paste, and chromocor compound crude product is freeze-dried to obtain at -80 DEG C；
（6）Chromocor compound crude product is dissolved in purified water, concentration 40mg/ml crosses the ethyl alcohol that 2~3 times of wet resin volumes are added in column
Solution elutes, 1.2~1.5ml/min of flow velocity, room temperature elution；
（7）By the solution decompression or vacuum concentration after elution, the solution after concentration is freeze-dried 18~24 hours at -80 DEG C and makes
Obtain honeysuckle extractive of general flavone.
2. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（2）The solid-liquid ratio of middle honeysuckle and petroleum ether is 1：10~1:20（g/ml）.
3. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（4）Middle filter residue is 1 with ethyl alcohol solid-liquid ratio:10~1:25（g/ml）.
4. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（4）Middle ethanol solution concentration is 40%~80%.
5. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（4）Middle to be extracted using Microwave-Assisted Ethanol solution, microwave temperature is 30~60 DEG C, 30~75 points of microwave irradiation time
Clock.
6. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（4）Middle to be extracted using Microwave-Assisted Ethanol solution, Microwave Extraction number is 2 ~ 3 times.
7. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（5）Middle filtrate is concentrated using vacuum or condition of negative pressure, and vacuum degree is -0.085~0.09MPa.
8. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（5）Middle filtrate is concentrated into the 20%~30% of material liquid.
9. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（6）Middle chromocor compound crude product is eluted using D101 macroreticular resins.
10. a kind of preparation method of honeysuckle extractive of general flavone as described in claim 1, which is characterized in that the step
（6）Middle chromocor compound crude product is eluted using 75% ~ 85% ethyl alcohol.
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| CN201810690091.4A CN108653369A (en) | 2018-06-28 | 2018-06-28 | A kind of preparation method of honeysuckle extractive of general flavone and its application in honey refines emblic loquat leaf extract |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113616744A (en) * | 2021-09-01 | 2021-11-09 | 山西大学 | Preparation method and application of millet whole grain flavone active component |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103027937A (en) * | 2012-05-28 | 2013-04-10 | 济宁医学院 | Method for extracting general flavone from honeysuckle leaves |
| CN107519227A (en) * | 2017-09-12 | 2017-12-29 | 临沂大学 | A kind of honeysuckle composition particle and preparation method thereof |
-
2018
- 2018-06-28 CN CN201810690091.4A patent/CN108653369A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103027937A (en) * | 2012-05-28 | 2013-04-10 | 济宁医学院 | Method for extracting general flavone from honeysuckle leaves |
| CN107519227A (en) * | 2017-09-12 | 2017-12-29 | 临沂大学 | A kind of honeysuckle composition particle and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 孔令义: "《中药制药化学》", 30 April 2007, 中国医药科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113616744A (en) * | 2021-09-01 | 2021-11-09 | 山西大学 | Preparation method and application of millet whole grain flavone active component |
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